Treatment of textile materials



. Patented Aug. 27, 1946 TREATMENT OF TEXTILE MATERIALS George W.Seymour and Walter Brooks, Cumberland, Md., assignors to CelaneseCorporation of America, a corporation of Delaware No Drawing.Application December 30, 1942, Serial N0. 470,662

8 Claims. (01. 252-835) This invention relates to the treatment oftextile materials and relates more particularly to the conditioning offibers and filaments made of organic derivatives of cellulose wherebythe same are rendered more amenable to textile operations such ascarding, drafting,- spinning and,

- also weaving or knitting, and to the formed yarns and fabrics madefrom or containing said organic derivatives of cellulose fibers orfilaments.

An object of the present invention is theprovision of an improved methodof preparing a stable liquid for conditioning fibers and filamentscomprising organic derivatives of cellulose to improve their amenabilityto textil operations such as carding, drafting, spinning, twisting,coning, pirning, hanking, weaving, knitting and the like.

A further object of our invention is to provide a treatment for textilefibers or filaments containing organic derivatives of cellulose with anovel conditioning fluid whereby they ar rendered more anti-static andhave the proper amount of friction between the fibers to give a controlto carding and drafting.

A further object of the present invention is to provide a process forthe treatment of organic derivatives of cellulose textile materials witha conditioning fluid containing different types of lubricants, softenersand other ingredients whereby fabrics made from such materials have asofter hand and present a uniform appearance. 7

Another object of the invention is the provision of an improved textilematerial made of or containing organic derivative of cellulose fibers orfilaments having applied thereto a conditioning fluid of the presentinvention.

Other objects of our invention will appear from the following detaileddescription and the appended claims.

Many substances such as vegetable, animal and mineral oils, both normaland specially treated, have been employed for lubricating orconditioning textile materials in order to render them more suitable forprocessing a fabric. While these substances have resulted in someimprovements in processing, they still left much to be desired and inaddition presented problems of their own. Thus, the oils tend to gum orpolymerize with time so that lubricated fibers and filaments cannot beprocessed uniformly dueto the hardening of the oil. Moreover, suchgumming or polymerization makes it diiiicult for the conditioning agentto beremoved from the fabrics made with such textile materials. Alsolubricating or conditioning compositions heretofore used did notpenetrate or spreadevenly into or upon the fibers or filaments treatedor presented other difficulties of applications.

Particularly in the case of conditioning of relatively short length orstaple fibers formed of organic derivatives of cellulos do the priorlubricating compositions fall short of what was de-,

sired. While some such compositions were capable of conditioning thefibers to withstand the numerous bendings and twistings imparted theretoduring processing, they did not impart the desired degree of frictionbetween the fibers to I enable them to be drawn or drafted to fineyarns. On the other hand, some compositions are satisfactory withrespect to their friction characteristic but do not properly conditionthe fibers for weaving, knitting or other textile operations.

We have found that these and other disadvantages arising' out of the useof known conditioning fluids can be avoided by the use of theconditioning fluid of the present invention comprising a mixture ofseveral ingredients, some of which react with each other. Fibers treatedwith our novel composition behave much more.

satisfactorily in carding and drafting operations and in subsequentwinding, twisting, warping, weaving, knitting and like operations thando untreated fibers and filaments, or fibers and filaments treated withknown conditioning fluids.

Moreover, we have found that fibers treated with our conditioning fluidsare not deleteriously affected upon storage and in some case may even beimproved after being stored for a time. Furthermore, the conditioningfiuid of our invention does not alter its effects on the fibers storedfor long periods of time but retains the same balance of friction forcarding and drafting operations, lubricative properties for othertextile operations and conditioning properties to withstand the rigorsof processing. Other advantages are also imparted to the yarn by ourconditioning fluid as will appear hereinafter.

In accordance with our invention we treat fibers or filaments containingorganic derivative of cellulose with a conditioning agent formed byreacting a mineral oil, a fatty acid and sulphuric acid and to thisreaction product adding a vege- *tabl'e oil, an alkali, an alkyloiamineand water.

This conditioning agent is stabilized, preserved against oxidation andgiven an enhanced covering power by the addition of an alkylated phenolor other spreading and penetrating agent.

The fibers or filaments to be treated in accordance 'withv thisinvention may have as a basis any suitable organic derivative ofcellulose such as organic esters of cellulose and cellulose ethers.

. Examples of organic esters of cellulos are cellu-' lose acetate,cellulose propionate and cellulose butyrate or mixed esters such ascellulose acetatebutyrate or cellulose acetate-propionate, while alsoemployed as the basis of the fibers or filaments.

This invention is applicable to the treatment of fine filaments,,or aplurality of such fine filav ments associated together in the form ofyarn, or larger filaments such as artificial bristles, horse- 1 hair,straw and the like; and also to fabrics or other articles formedtherefrom. It, is, particularly applicable to the treatment ofrelatively short lengths of fibers, say from inch to 6 or 1 more inchesin length that are known in the trade as staple fibers. The conditioningliquid may be applied to the staple fibers or to the continuousfilaments from which the staple fibers are cut or j to the filaments asthey are-being cut. The fibers or'fllaments need not consist wholly offibers or filaments of organic derivative of cellulose but may containfibers of other materials such as natural silk; artificial fibers ofreconstituted cellulose, wool, cotton, etc. The conditioning liquid ofthe present invention may be employed j on artificial fibers thatcontain finely divided pigment-like materials that alter the lustreand/or color of the fiber without deleterious effect.

As stated above, our novelconditioning fluid 1 comprises the reactionproduct of mineral oil, fatty acid and sulphuric acid, which reactionproduct is reacted with a raw vegetable oil, an alkali, an alkylolamineand water and the whole' 1 resulting compound stabilized and otherwiseimproved by the addition of an alkylated phenol, 1 or where the fibersto be treated contain an ester of cellulose with an alkylated phenoland/or esterified vegetable oil. In a preferred form of our inventionall or a part of the raw vegetable;

oil is added with the fatty acid and takes part in the first reaction.Other materials may also be added, such as, for example, softeners forparticular fibers being treated; substances which aid in emulsifying thecom-position and also facilitate the removal of the same by scouring;preservatives' such as Dowicide A (sodium ortho phenyl phenate), etc.Fugitive dyes or tints may also be added to identify the materials inprocessing also permanent dyes, etc. may be added.

The mineral oil employed in forming the conditioning liquid of ourinvention may be one having a. paraflinic or naphthenic base and aviscosity of 50 to 75 seconds. The viscosity referred, to herein isSaybolt Universal at 100 F. However, the viscosity of the mineraloilemployed is deter mined by the over-all viscosity desired in the ofviscosity of the mineral oil is set by the-over-.

conditioning liquid or, in other words, the limit all viscosity of theconditioning liquid which dried on the fibers gives desirable textilecharacteristics thereto. This over-all viscosity may be on the order of80 to 200 seconds and preferably about 150 seconds. Optimum results areobtained using a white mineral oil having a paraiilnic base i and aviscosity of 50seconds.

The fatty acid employed in'the first reaction step of ourinvention maybe any suitable fatty acid, examples of which are oleic acid, recinoleicacid, palmitic acid, etc. The preferred fatty acid, however, is oleicacid of at least 'technical grade or better. The sulphuric acid employedis fuming sulphuric acid containing about 20% SO: and is commonly termedOleum 20%.

; A preferred method of preparing the condition ing fluid of ourinvention is as follows:

10 About 29 parts of a white mineral oil of 50 vis- 1, cosity, 21.5parts of oleic acid or its equivalent of other fatty acids and 10.5parts of raw vegetable oil such as olive oil, rice oil or peanut oil aremixed and "cooled to about 10 C. in a; jacketed l5 mixer through thejacket of which circulates a cooling medium having a temperature of --10to C. With constant stirring about 6.5 parts of fumingsulphuric acid areslowly added, say in a 30 minute period. The temperature rises to 20about 20 C. du'ring'the reaction time of about 75 minutes. h

To the above reaction product is-adde'd about .parts. of diamyl phenoland then "a mixture of about 11.6 parts of triethanolamine or itsequivalent of other alkylolamine, 1.6 parts of sodium hydroxide or itsequivalent of potassium hydroxide and 14 parts of water. The whole batchis stirred until all reaction ceasesand a clear oil'is formed. Some ofthe raw vegetabl oil may be added with the alkali, if so desired. Thiconditioning liquid may be mixed with water and applied as an emulsionto the fibers, filaments, yarns. etc. In the resulting productsubstantially 40% of the original oleic or equivalent fatty acid issulfated and/or sulfonated; substantially 9% of the original rawvegetable oil is sulfated and/or sulfonated; the mineral oil remainssubstantially unaffected chemically; none of the vegetable oil issaponifiedby the alkali and triethanolamine which has been added inamounts to neutralize all the sulfuric acid present and most but not allof the oleic or other fatty acid used. The product is slightly acid dueto the presence of about 10% of umieutralized oleic acid.

The product is an oily compound which readily forms a stable, whiteemulsion in water, 2% emulsian'thereof having a pH of 6.8. In place ofall or a part of the diamyl pheno employed in the above formula theremay be substituted other alkyl derivatives of phenols; The alkylatedphenol not only acts as an anti-oxident but also enhances thepenetrative and spreading .eflects of the. conditioning liquid in and onthe fibers and yarns and stabilizes the conditioning ponents uponstanding. Examples of other alkyl derivatives of. phenols or alkylatedphenols are dibutyl and 'diamyl derivatives of cresols and xylenols, thedibutyl and diamyl derivatives of any of the mono-chlorophenols, etc.The diamyl tricresyl phosphate ortriphenyl phosphate or similarcompounds. When the fiber or yarn being treated contains organic esters,of cellulose, the addition of an acetylated vegetable oil, such asacetylated castoror oilve oil, may be employed advantageously.These-agents although having several functions are called, for thepurpose of simplifyingthe description of the invention, spreading andpenetrating agents. 4 In. place of all or a partof the'triethanolaminetheremay be substituted otherjhydroxylated amines such as'monoethanolamine, diethanolamine, iliethylamino ethanol, .ethyldiethanolamine, amethyl-z -amino'propanol, etc.

liquid whereby it does not separate into it comphenol may alsobereplaced in whole. or in part by be varied to some degree, dependingsomewhat on the use to which the treated fibers ar to be put and theproperties which it is desired to emphas'ize. Thus; where it is desiredto increase the spreading, and wetting properties the amount of diamylphenol may be increased from 5 parts to or more parts. Also the amountof mineral oil may be varied from 20 parts to 35 parts depending on thelubricity desired. Also the amount of alkali and alkylolamines may bevaried. In this respect we have found that the preferred conditioningliquid should be one that a 2% emulsion of same in water has a pH offrom 6.6 to '7.

The conditioning liquid obtained in accordance with our invention may beapplied to fibers and filaments in the concentrated form or it may beapplied as an emulsion, or dissolved or suspended in a carrier. Theamount of conditioning liquid applied may vary from 1 to 10 or more percent based on the weight of the untreated fibers. The conditioningliquid is preferably applied to running yarns and filaments by wicks,rollers or other furnishing devices. However, it may also be applied tofibers by dipping bales thereof in a bath of the conditioning liquid orby. spraying the same with a mistof some.

-'I'he term sulfonation" as used in the appended claims designates notonly the phenomenon of sulfonation proper (that is the formation ofproducts wherein sulfur atoms are linked directly to carbon atoms) butalso sulfati'on (thatis the formation of products wherein the sulfuratoms are linked to oxygen atoms that are in turn linked to carbonatoms).

tailed description is given merely by way-of illustration and that manyvariations may e made therein without departing from the spirit of ourinvention.

Having described our invention, what we desire to secure by LettersPatent is:

.1. Process for the preparation of a conditioning liquid for textilematerials which comprises reacting a mixture comprising a mineral oil, avegetable oil, a higher fatty-acid and fuming sulphuric acid at atemperature no greater than about 20 C. whereby sulphonation of at leastpart of the fatty acid and vegetable oil occurs and then adding aspreading and penetrating agent and an amount of alkali-metal hydroxideand an alkylolamine to neutralize all of the sulfuric acid and the majorportion of the higher fatty acid.

2. Process for the preparation of a conditioning liquid for textilematerials which comprises reacting a mixture comprising a mineral oil, avegetable oil, a higher fatty acid and fuming sulphuric acid at atemperature no greater than about 20 0. whereby sulphonation of at leastpartof the fatty acid and vegetable oil occurs and then adding analkylated phenoland an amount of alkali-metal hydroxide and analkylolamine to neutralize all of the sulfuric acid and the majorreacting a mixture comprising a mineral oil, a vegetable oil, ahigherfatty acid and fuming sulphuric acidat a temperature no greater thanabout 20 C. whereby sulphonation of at least part of the fatty acid andvegetabl oil occurs and then adding diamyl phenol and an amount ofalkali-metal hydroxide and an alkylolamine to neutralize all of thesulfuric acid and the a major portion of the higher fatty acid.

4. Process for the preparation of a conditioning liquid for textilematerials whicncomprises reacting a mixture comprising a mineral oil, a,

vegetable oil, a higher-fatty acid and fuming sulphuric acid at atemperature no greater than about 20 C. whereby sulphonation of at leastacid at a temperature no greater than about 20 C. whereby sulphonationof at least part of the fatty acid and vegetable oil occurs and thenadding a spreading and penetrating agent and an amount of alkali-metalhydroxide and an alkylolamine to neutralize all of the sulfuric acid andthe major portion of the higher fatty acid.

6. Process for the preparation of a conditioning liquid for textilematerials which comprises reacting a mixture comprising a mineral oil, avegetable oil, oleic acid and fuming sulphuric acid at a temperature nogreater than about 20 C.

whereby sulphonation ofat least'part of the fattyacid and vegetable oiloccurs and then adding diamyl phenol and an amount of alkali-metalhydroxide and an alkylolamine to neutralize all of the sulfuric acid andthe major portion of the higher fatty acid.

7. Process for the preparation of a conditioning liquid for textilematerials which comprises reacting a mixture comprising a mineral oil, avegetable oil, oleic acid and fuming sulphuric acid at a temperature nogreater than about 20 0. whereby sulphonation of at least part of thefatty acid and vegetable oil occurs and then adding an acetylated castoroil and an amount of alkalimetal hydroxide and an alkylolamine toneutralize all of the sulphuric acid and the major portion'of the higherfatty'acid.

8. Process for the preparation of a conditioning liquid for textilematerials which comprises reacting a mixture comprising a mineral oil.raw

peanut oil, oleic acid and fuming sulphuric acid at a temperature nogreater than about 20 C. whereby sulphonation of at least part of thefatty acid and vegetable oil occursand thenadding a spreading andpenetrating agent and an amount of alkali-metal hydroxide and analkylolamine to neutraliz all of the sulphuric acid and the maiorportion'of the higher fatty acid.

GEORGE W. SEYMOUR.

